반응 #710532

ord-1a7fd1c2999b4aaa89245faa1cdccc57

반응 방정식

CS(=O)(=O)O
Methanesulfonic acid
CC(C)(C)OC(=O)N1CCC[C@H](C(=O)O)C1
(S)—N-(tert-butoxycarbonyl)nipecotic acid
CCN(CC)CC
Triethylamine
O=C(O)[C@H]1CCCNC1
titled compound
O=C(O)[C@H]1CCCNC1
(S)-nipecotic acid

반응 조건

온도
25°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타solid was precipitated
  2. 2
    기타The solid was sufficiently precipitated
  3. 3
    workup.STIRRINGthe solution was stirred at 25° C. for 30 minutes
  4. 4
    기타Thereafter, the solid was separated by filtration under reduced pressure
  5. 5
    세척The solid was washed with methylene chloride (5 mL)
  6. 6
    기타drying

실험 절차

Methanesulfonic acid (576 mg, 6 mmol) was added to a solution of (S)—N-(tert-butoxycarbonyl)nipecotic acid (1145 mg, 5 mmol) and methylene chloride (5 mL), and the mixture was stirred at 25° C. for 16 hours. Triethylamine (708 mg, 7 mmol) was added thereto, and then solid was precipitated. The solid was sufficiently precipitated, and then the solution was stirred at 25° C. for 30 minutes. Thereafter, the solid was separated by filtration under reduced pressure. The solid was washed with methylene chloride (5 mL), and then was subjected to vacuum drying. Thereby, the titled compound was produced as a white solid (238 mg, yield of 37%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09302980B2uspto-grants-2016_04